CN104310573A - Combination electrode preparation method and application of combination electrode preparation method in bioelectricity Fenton system - Google Patents
Combination electrode preparation method and application of combination electrode preparation method in bioelectricity Fenton system Download PDFInfo
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- CN104310573A CN104310573A CN201410665810.9A CN201410665810A CN104310573A CN 104310573 A CN104310573 A CN 104310573A CN 201410665810 A CN201410665810 A CN 201410665810A CN 104310573 A CN104310573 A CN 104310573A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F3/00—Biological treatment of water, waste water, or sewage
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry
Abstract
The invention discloses a combination electrode preparation method and the application of the combination electrode preparation method in a bioelectricity Fenton system, and belongs to the field of environmental engineering and waste water treatment. According to a combination electrode prepared through the combination electrode preparation method, a bioelectrochemistry system serves as a reactor to treat azo dye waste water, anode electro-microorganisms oxidize organic matter so that electrons and protons can be generated, the electrons and the protons are transferred to a cathode chamber through an external circuit and an ion exchange membrane, H2O2 is generated on a cathode in an in-situ mode with O2 as the electron acceptor, a cathode iron source is slowly released, Fenton reaction is performed between iron and H2O2 generated in the in-situ mode, and thus non-biodegradable pollutants are treated.
Description
Technical field
The present invention relates to a kind of preparation of combined electrode and the application in bioelectricity Fenton system thereof, belong to environmental engineering and field of waste water treatment.
Background technology
Along with the development of printing and dyeing industry, the quantity discharged of waste water from dyestuff is increasing, and face of polluting is also more and more wider, has become one of topmost pollution source of water body.Azoic dyestuff occupies 80% of organic dye, and wastewater discharge is large, complicated component, belongs to used water difficult to degradate.
At present, the method that azo dye wastewater process adopts mainly comprises: Physical, biological process, chemical method three major types.Physical mainly comprises absorption method and membrane separation process, and it utilizes physical action to be separated from waste water by azoic dyestuff, then reclaims or advanced treatment it.Although the method has better treatment effect to most of waste water from dyestuff, realize water resources recycling, there is cleaning difficulty, easily block, easily pollute, the shortcomings such as regeneration expense is high.Biological process utilizes the metabolism of microorganism to decompose and organism in conversion of waste water, but aerobic method power consumption is large, mud generation is large, the organic pollutant of process complex structure and high density is difficult to reach standard, anaerobic process microbiological anaerobic accretion rate is slow, container volume is large, and the residence time is long, and independent employing is also difficult to reach emission standard.Chemical method mainly comprises coagulant sedimentation, oxidation style, electrochemical process etc., and method cost is high, and oxidation technology is applicable to and other technologies coupling process waste water, and electrochemical process is higher for equipment requirements, thus can not be widely used.
Fenton (Fenton) and BES (bioelectrochemical system) combine by the present invention, anode electrogenesis microorganism can utilize organic substrates to produce electronics and proton, the electronics produced is passed to cathode surface by wire, proton then enters in cathode compartment by ion-exchange membrane, electronics and proton then with O
2be combined in negative electrode in-situ preparation H
2o
2; Combined electrode is then negative electrode, and source of iron slowly releases, can with the H produced
2o
2fenton's reaction occurs, and this system combined both can produce electric energy, can realize again the process of negative electrode to Recalcitrant chemicals.
Summary of the invention
First technical problem that the present invention will solve is to provide a kind of preparation method of combined electrode, mainly comprises the following steps:
(1) washing, carbon oxide fiber: with washing composition backflow washing carbon fiber 8-10h, remove the oxidation of impurities product of carbon fiber surface absorption, take out in 60-80 DEG C of oven dry to constant weight; Use oxidizing carbon fiber, interval agitation of solutions; Take out carbon fiber, with deionized water washing by soaking 3-5 time, in 60-80 DEG C of oven dry to constant weight;
(2) combined electrode is prepared: the activated carbon fiber of peroxidation process of learning from else's experience immerses in iron salt solutions, 30 DEG C, 40KHz supersound process 0.5-2h, with peristaltic pump, metal boride solution is joined in above-mentioned system, make molysite and metal boride molar concentration rate 1:5-1:3 in system, after abundant reaction reduction molysite, repeatedly rinse carbon fiber 3-5 time with deionized water, dry to constant weight in 60-80 DEG C, this carbon fiber titanium silk of 15-25g is fixedly made combined electrode.
In one embodiment of the invention, the washing composition that step (1) adopts is ethanol acetone or benzene or water.
In one embodiment of the invention, the oxygenant that step (1) adopts is acid potassium bichromate or concentrated nitric acid or concentrated sulfuric acid solution.
In one embodiment of the invention, step (1) adopts acid potassium bichromate or concentrated nitric acid or concentrated sulfuric acid solution in 80-120 DEG C of carbon oxide fiber 1-3h.
In one embodiment of the invention, the mass ratio of step (1) carbon fiber and oxygenant is 1:40-1:50.
In one embodiment of the invention, step (1) washing, carbon oxide fiber: use ethanol acetone or benzene or aqueous solution backflow to wash carbon fiber 8-10h, remove the oxidation of impurities product of carbon fiber surface absorption, take out in 60-80 DEG C of oven dry for subsequent use to constant weight subsequently; With acid potassium bichromate or concentrated nitric acid or concentrated sulfuric acid solution carbon oxide fiber, interval agitation of solutions, the mass ratio of carbon fiber and oxygenant is 1:40-1:50; Take out carbon fiber, with deionized water washing by soaking 3-5 time, in 60-80 DEG C of oven dry to constant weight.
In one embodiment of the invention, step (1) the ethanol acetone soln backflow washing carbon fiber 10h of volume ratio 1:1, avoid the oxidation products of impurity to be adsorbed on carbon fiber surface and affect its quality, take out in 80 DEG C of oven dry for subsequent use to constant weight subsequently; In the stink cupboard that return line is housed, with acid potassium bichromate solution (in mass ratio, containing 20%K
2crO
7, 30%H
2sO
4) heated constant temperature carrys out carbon oxide fiber, oxidization time is 2h, and oxidizing temperature is 80 DEG C, and every 20min shakes a solution, and carbon fiber and oxygenant mass ratio are 1:50; Take out carbon fiber, with deionized water washing by soaking 5 times, dry to constant weight in 80 DEG C.
In one embodiment of the invention, the molysite that step (2) adopts is FeCl
36H
2o.
In one embodiment of the invention, the metal boride that step (2) adopts is NaBH
4.
In one embodiment of the invention, step (2) prepares combined electrode: get 3-9g through the activated carbon fiber of oxide treatment and immerse FeCl
36H
2in O solution, 30 DEG C, 40KHz supersound process 0.5-2h, with peristaltic pump by NaBH
4solution adds in iron-containing liquor, makes FeCl in system
36H
2o and NaBH
4molar concentration rate 1:5-1:3, fully after reduction molysite, repeatedly rinses 3-5 time with deionized water, dries to constant weight, this carbon fiber titanium silk of 15-25g is fixedly made combined electrode in 60-80 DEG C.
In one embodiment of the invention, step (2) is by the FeCl of 3g through the gac immersion 3g/L of oxide treatment
36H
2in O solution, by this solution 30 DEG C, 40KHz supersound process 1h, with the NaBH of peristaltic pump by 15g/L
4solution adds in iron-containing liquor, fully after reaction, repeatedly rinses 5 times with deionized water, dries to constant weight, this carbon fiber titanium silk of 20g is fixedly made combined electrode in 80 DEG C.
Second technical problem that the present invention will solve is to provide a kind of bioelectrochemical system reaction unit containing described combined electrode, and described reaction unit comprises anode carbon brush, negative electrode carbon brush, reference electrode, cationic exchange membrane, external resistance, water inlet interface, water outlet mouthpiece and fresh feed pump; Reaction unit is divided into room, negative and positive the two poles of the earth by cationic exchange membrane, the material of cathode and anode room is all synthetic glass, anode carbon brush is the common carbon brush of titanium silk and carbon fiber composition, negative electrode carbon brush is combined electrode, anolyte compartment's top drilling is for placing reference electrode, bottom side and top has water-in and water outlet, and anode and cathode and reference electrode form external circuit by wire, and centre is connected with the resistance of 100 Ω.
In one embodiment of the invention, described cathode and anode room volume is 550mL, and external diameter is 9cm, internal diameter 7cm, is highly 14cm.
Described anolyte compartment is the electrogenesis nutritive medium of 3:1 and the anaerobic sludge supernatant liquor through the domestication of electrogenesis nutritive medium built with volume ratio, and when anode potential is stabilized in-0.5V, anode is tamed successfully.The formula (mg/L) of described electrogenesis nutritive medium: KCl 0.13, NH
4cl 0.31, NaH
2pO
42.7, Na
2hPO
411.55, anhydrous sodium acetate 1.0, micro-1mL/mL, VITAMIN liquid 1mL/mL.Wherein, trace element formula (g/L): nitrilotriacetic acid(NTA) 1.5, MgSO
47H
2o 3.0, MnSO
4h
2o 0.5, NaCl 1.0, FeSO
47H
2o 0.1, CoCl 0.1, CaCl
20.1, ZnSO
47H
2o 0.1, CuSO
45H
2o 0.01, potassium aluminium alum 0.01, H
3bO
50.01, Na
2moO
40.01; VITAMIN liquid formula (mg/L): vitamin H 2.0, Lin Suanna Vitamin B2 Sodium Phosphate .0, pyridoxine hydrochloride 10.0, vitamins B
15.0, vitamins B
25.0, nicotinic acid 5.0, D-acid calcium 5.0, vitamins B
120.1, para-amino benzoic acid 5.0, Thioctic Acid 5.0.
When described bioelectrochemical system reaction unit is applied to dye wastewater treatment, anode electrogenesis microorganism utilizes organic substrates to produce electronics and proton, produce electronics be passed to cathode surface by wire, proton then enters in cathode compartment by ion-exchange membrane, electronics, proton then with O
2be combined in negative electrode in-situ preparation H
2o
2; Combined electrode is negative electrode, slow releasing source of iron, with the H produced
2o
2there is Fenton's reaction, realize the process to Recalcitrant chemicals.Eliminate additional source of iron, increase the service life, and lifting sewage treatment effect.
H is there is in tradition Fenton's reaction
2o
2the shortcoming such as costly, easily to decompose, side reaction is many, the present invention adopts bioelectricity Fenton technology, makes H
2o
2in-situ preparation becomes possibility, utilizes the combined electrode of preparation simultaneously, makes negative electrode source of iron slow releasing, has deducted additional source of iron, accelerates sewage disposal speed, and extends electrode life.Not only simple to operate, be easy to control, and improve treatment effect, can not secondary pollution be produced, reduce reaction cost.
Accompanying drawing explanation
Fig. 1 is indication bioelectricity Fenton system dye wastewater treatment process unit structural representation of the present invention; 1, anode carbon brush; 2, negative electrode carbon brush; 3, reference electrode; 4, cationic exchange membrane; 5, external resistance; 6, water inlet interface; 7, water outlet mouthpiece; 8, fresh feed pump.
Fig. 2 is that bioelectrochemical system put into by common carbon brush and combined electrode, the comparison diagram of methyl orange solution degraded.
Embodiment
The preparation of embodiment 1 combined electrode
In apparatus,Soxhlet's, be the ethanol acetone soln backflow washing carbon fiber 10h of 1:1 by volume ratio, avoiding the oxidation products of impurity to be adsorbed on carbon fiber surface affects its quality, takes out in 80 DEG C of oven dry for subsequent use to constant weight subsequently.In the stink cupboard that return line is housed, with acid potassium bichromate solution heated oxide carbon fiber, oxidization time is 1-3h, and oxidizing temperature is 80-120 DEG C, and every 20min shakes a solution, and carbon fiber and oxygenant mass ratio are 1:50.Take out carbon fiber, with deionized water washing by soaking 5 times, dry to constant weight in 80 DEG C.
Get the FeCl of 3g through the gac immersion 3g/L of oxide treatment
36H
2in O solution, by this solution in 30 DEG C, 40KHz supersound process 1h, with the NaBH of peristaltic pump by 15g/L
4solution adds in iron-containing liquor, FeCl
36H
2o and NaBH
4molar concentration rate 1:5, fully after reduction molysite, repeatedly rinses 5 times with deionized water, dries to constant weight, this carbon fiber titanium silk of 20g is fixedly made combined electrode in 80 DEG C.
Embodiment 2 puts into bioelectrochemical system dye wastewater treatment by preparing combined electrode
1,2 be described as follows by reference to the accompanying drawings:
As shown in Figure 1, the present invention is using bioelectrochemical system as reactor, and this reactor is made up of cathode and anode room, and centre is separated by cationic exchange membrane.Negative electrode utilizes peristaltic pump from water-in (6) water inlet, and sampling is then by water outlet 7, and the catalyzer of electrogenesis microorganism and iron is attached on carbon brush (1), (2) respectively.
First, inoculating in the anode compartment into cumulative volume is electrogenesis nutritive medium and the anaerobic sludge supernatant liquor of 550mL, wherein the volume ratio of electrogenesis nutritive medium and anaerobic sludge supernatant liquor (containing electrogenesis microorganism) is 3:1, and anaerobic sludge takes from Wuxi north of the city sewage work.Wherein electrogenesis microorganism supernatant liquor absorbancy under 600nm wavelength, between 0.021-0.025, starts device of the present invention at ambient temperature.When anode potential is stabilized in-0.5V, anode is tamed successfully.
As shown in Figure 2, cathode compartment uses combined electrode and common carbon brush respectively.In cathode compartment, add the common 550mL simulated wastewater containing 5mg/L tropeolin-D, with the Na of 0.05mol/L simultaneously
2sO
4for electrolytic solution.Cathode compartment uses the reactor of common carbon brush to add the FeSO of 0.1g/L
47H
2o, every 15min get a sample.Use methyl orange degradation in the reactor of combined electrode very fast in 2 hours, last real-time concentration and starting point concentration ratio (C/C
0) be 0.157, namely tropeolin-D clearance reaches 84.3%.As can be seen here, combined electrode is remarkable to the removal effect of tropeolin-D in bioelectricity Fenton system.
Cathode compartment uses the combined electrode of combined electrode and not oxidised process respectively, as stated above treatment of simulated waste water.Result shows, compares the present invention through oxide treatment then in conjunction with the combined electrode of iron, and when adopting the combined electrode of not oxidised process, in 2 hours, methyl orange degradation speed obviously declines, last real-time concentration and starting point concentration ratio (C/C
0) reaching 0.423, tropeolin-D clearance is only 57.7%.
Combined electrode, common carbon brush are reused 6-7 time as stated above, when negative electrode adopts combined electrode, methyl orange degradation speed slightly declines with when using first, and when negative electrode adopts common carbon brush, methyl orange degradation speed significantly declines.
Although the present invention with preferred embodiment openly as above; but it is also not used to limit the present invention, any person skilled in the art, without departing from the spirit and scope of the present invention; all can do various changes and modification, what therefore protection scope of the present invention should define with claims is as the criterion.
Claims (10)
1. a preparation method for combined electrode, mainly comprises the following steps:
(1) washing, carbon oxide fiber: with washing composition backflow washing carbon fiber 8-10h, remove the oxidation of impurities product of carbon fiber surface absorption, take out in 60-80 DEG C of oven dry to constant weight; Use oxidizing carbon fiber, interval agitation of solutions; Take out carbon fiber, with deionized water washing by soaking 3-5 time, in 60-80 DEG C of oven dry to constant weight;
(2) combined electrode is prepared: the activated carbon fiber of peroxidation process of learning from else's experience immerses in iron salt solutions, 30 DEG C, 40KHz supersound process 0.5-2h, with peristaltic pump, metal boride solution is joined in above-mentioned system, make molysite and metal boride molar concentration rate 1:5-1:3 in system, after abundant reaction reduction molysite, repeatedly rinse carbon fiber 3-5 time with deionized water, dry to constant weight in 60-80 DEG C, this carbon fiber titanium silk of 15-25g is fixedly made combined electrode.
2. method according to claim 1, it is characterized in that, step (1) uses ethanol acetone or benzene or aqueous solution backflow to wash carbon fiber 8-10h, avoids the oxidation products of impurity to be adsorbed on carbon fiber surface, takes out in 60-80 DEG C of oven dry for subsequent use to constant weight subsequently; With acid potassium bichromate or concentrated nitric acid or concentrated sulfuric acid solution in 80-120 DEG C of carbon oxide fiber 1-3h, interval agitation of solutions, the mass ratio of carbon fiber and oxygenant is 1:40-50; Take out carbon fiber, with deionized water washing by soaking 5 times, dry to constant weight in 80 DEG C.
3. method according to claim 1, is characterized in that, 3-9g is immersed FeCl through the gac of oxide treatment by step (2)
36H
2in O solution, by this solution supersound process 1h, with peristaltic pump by NaBH
4solution adds in iron-containing liquor, fully after reaction, repeatedly rinses 3-5 time with deionized water, dries to constant weight, this carbon fiber titanium silk of 15-25g is fixedly made combined electrode in 60-80 DEG C.
4. according to the combined electrode that the arbitrary described method of claim 1-3 prepares.
5. the bioelectrochemical system reaction unit containing combined electrode described in claim 4, it is characterized in that, described reaction unit comprises anode carbon brush, negative electrode carbon brush, reference electrode, cationic exchange membrane, external resistance, water inlet interface, water outlet mouthpiece and fresh feed pump; Reaction unit is divided into room, negative and positive the two poles of the earth by cationic exchange membrane, the material of cathode and anode room is all synthetic glass, anode carbon brush is the common carbon brush of titanium silk and carbon fiber composition, negative electrode carbon brush is combined electrode, anolyte compartment's top drilling is for placing reference electrode, bottom side and top has water-in and water outlet, and anode and cathode and reference electrode form external circuit by wire, and centre is connected with resistance.
6. reaction unit according to claim 5, is characterized in that, described cathode and anode room volume is 550mL, and external diameter is 9cm, internal diameter 7cm, is highly 14cm.
7. reaction unit according to claim 5, is characterized in that, described anolyte compartment is the electrogenesis nutritive medium of 3:1 and the anaerobic sludge supernatant liquor through the domestication of electrogenesis nutritive medium built with volume ratio, and when anode potential is stabilized in-0.5V, anode is tamed successfully.
8. reaction unit according to claim 7, is characterized in that, described electrogenesis nutritive medium contains by mg/L: KCl0.13, NH
4cl 0.31, NaH
2pO
42.7, Na
2hPO
411.55, anhydrous sodium acetate 1.0, micro-1mL/mL, VITAMIN liquid 1mL/mL; Wherein, trace element by the formula of g/L is: nitrilotriacetic acid(NTA) 1.5, MgSO
47H
2o 3.0, MnSO
4h
2o 0.5, NaCl 1.0, FeSO
47H
2o 0.1, CoCl 0.1, CaCl
20.1, ZnSO
47H
2o 0.1, CuSO
45H
2o 0.01, potassium aluminium alum 0.01, H
3bO
50.01, Na
2moO
40.01; VITAMIN liquid by the formula of mg/L is: vitamin H 2.0, vitamins B 2.0, pyridoxine hydrochloride 10.0, vitamins B
15.0, vitamins B
25.0, nicotinic acid 5.0, D-acid calcium 5.0, vitamins B
120.1, para-amino benzoic acid 5.0, Thioctic Acid 5.0.
9. the application method of bioelectrochemical system reaction unit according to claim 7 in dye wastewater treatment.
10. method according to claim 9, it is characterized in that, anode electrogenesis microorganism utilizes organic substrates to produce electronics and proton, and the electronics of generation is passed to cathode surface by wire, proton then enters in cathode compartment by ion-exchange membrane, electronics, proton then with O
2be combined in negative electrode in-situ preparation H
2o
2; Combined electrode is negative electrode, slow releasing source of iron, with the H produced
2o
2there is Fenton's reaction, realize the process to Recalcitrant chemicals.
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